反应详情

To a solution of (3aR*,10aS*)-9-benzyl-4-(chloroacetyl)-2,3,3a,4,9,10a-hexahydrobenzo[b]-cyclopenta[e][1,4]diazepin-10(1H)-one (1.0 g, 2.7 mmol) and benzylamine (1.45 g, 13.6 mmol) in ethanol (30 mL) was added potassium carbonate (560 mg, 4.1 mmol), and the mixture was refluxed for 17 hours. The solvent was distilled off. To the residue was added water, which was subjected to extraction with dichloromethane. The extract was washed with water, dried and, then, the solvent was distilled off. The residue was purified by silica-gel column chromatography (ethyl acetate-hexane 1:1), followed by crystallization from diethyl-ether to give 0.36 g (yield 30%), m.p. 95-98° C.

1. temperaturethe mixture was refluxed for 17 hours
2. distillationThe solvent was distilled off
3. additionTo the residue was added water, which
4. extractionwas subjected to extraction with dichloromethane
5. washThe extract was washed with water
6. customdried
7. distillationthe solvent was distilled off
8. customThe residue was purified by silica-gel column chromatography (ethyl acetate-hexane 1:1)
9. customfollowed by crystallization from diethyl-ether
10. customto give 0.36 g (yield 30%), m.p. 95-98° C.